CN105668564A - Method for preparing biological activated carbon by hydrothermal carbonization of algae residue/algae sludge - Google Patents
Method for preparing biological activated carbon by hydrothermal carbonization of algae residue/algae sludge Download PDFInfo
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- CN105668564A CN105668564A CN201610032072.3A CN201610032072A CN105668564A CN 105668564 A CN105668564 A CN 105668564A CN 201610032072 A CN201610032072 A CN 201610032072A CN 105668564 A CN105668564 A CN 105668564A
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Abstract
The invention discloses a method for preparing biological activated carbon by hydrothermal carbonization of algae residue/algae sludge.The method includes the following steps: (1) mixing the algae residue/algae sludge with water prior to putting the mixture into a reaction kettle, performing heating reaction under the pressure less than 6 MPa and at the temperature of 160-220 DEG C for 2-20 hours, and naturally cooling to the room temperature; (2) subjecting a hydrothermal product obtained in the step (1) to filtration or centrifugal separation to obtain solid, and washing the solid; (3) drying the product obtained after washing in the step (2) at the temperature of 50-60 DEG C to obtain the biological activated carbon.Plenty of algae residue can be disposed highly efficiently as well as be utilized to turn waste into treasure; harm brought by the algae residue and algae toxins is reduced, and high efficiency and environmental friendliness are realized.
Description
Technical field
The present invention relates to environmental conservation and technical field of biological material, be specifically related to a kind of method that biological activated carbon is prepared in hydro-thermal carbonization utilizing algae-residue/algae mud.
Background technology
In recent years, the large-scale shallow water lake blue algae wawter bloom caused due to environmental pollution is frequently broken out and has been caused common concern. During breakout of cyanobacteria blooms, the water surface is covered by a thick layer of aeruginous water bloom, piles up along with wind direction migrates to bank, gives off an unpleasant smell after rotting. Series of new technology is developed for emergency processing blue-green alga bloom, such as artificial salvaging, machinery is salvaged, directly filter, flocculation or coagulating sedimentation, air supporting etc., brings another one problem while applying these technical finesse blue-green alga blooms, how to dispose and collects the algae-residue that substantial amounts of water content is high, contaminative is strong obtained. 2007 so far, only removes the gross weight of cyanophyceae from Taihu Lake up to 140.5 ten thousand tons (weight in wet bases). Due to algae-residue water content high (more than 90%), general algae-residue volume is process the water yield about 0.04%. Cyanophyceae utilize mucilage secretion assemble agglomerating cause dehydration difficulty, bulky, transport, placement and intractability are high, algae-residue discharges poisonous and harmful or offensive gases in decay process and discharges cyanophycean toxin in a large amount of cell simultaneously, in algae-residue, nitrogen phosphorus element content is up to 63mg/g, 9mg/g, deals with improperly and can be back in water source with runoff, cause secondary pollution. Therefore, the algae aqueous mixtures of the high concentration that algae-residue or collection obtain should suitable process or disposal in addition.
At present, the process of algae-residue or high concentration algae water or algae mud is mainly included following several measure: make fertilizer or feedstuff, extract active substance, produce biogas or preparation biodiesel etc. In algae-residue generating etc., make exploratory study additionally, domestic, but also not yet form industrialization. But, by still few for the research that algae-residue/algae mud is used for the fields such as chemical fertilizer, pesticide, environmental protection.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, it is provided that a kind of can efficiently dispose a large amount of algae-residue while can utilize again algae-residue, turn waste into wealth; Reduce the harm that algae-residue and Algae toxins bring, be also the hydro-thermal carbonization utilizing algae-residue/algae mud of the high-efficiency environment friendly method of preparing biological activated carbon simultaneously.
The present invention solves above-mentioned technical problem by techniques below means: a kind of method that biological activated carbon is prepared in hydro-thermal carbonization utilizing algae-residue/algae mud, comprises the following steps:
(1) algae-residue/algae mud is mixed with water insert in reactor, at pressure less than 6MPa, 160 DEG C～220 DEG C reacting by heating 2～20 hours, naturally cool to room temperature;
(2) being filtered or centrifugation by the hydrothermal product in step (1), the solid obtained washs;
(3) product after the washing in step (2) is dried process at 50 DEG C～60 DEG C, obtains biological activated carbon.
Preferably, described algae-residue/algae mud be by manually salvaging, machinery is salvaged, directly filtered, flocculation, coagulating sedimentation or pneumatically supported method obtain algae and water break out high concentration algae aqueous mixtures or the algae mud of generation.
Preferably, the water content of algae-residue/algae mud is 80%～95%, and the mass volume ratio of algae-residue/algae mud and water is 1:(0～3).
Preferably, algae-residue/algae mud is 3:1 or 2:1 or 1:1 or 1:2 with the mass volume ratio of water.
Preferably, described algae-residue/algae mud is the product by obtaining after filtering and concentrating.
Preferably, by Algae culture solution 400ml centrifugal 10min when 10000 turns, abandon supernatant and collect precipitation, resuspended with 40ml deionized water, obtain product.
Preferably, described algae-residue/algae mud is the solid by-product obtained in the algae-residue dried or algae bio diesel oil refining process; The solid by-product obtained in described dry algae-residue or algae bio diesel oil refining process and the mass volume ratio of water are 5%～200%.
Preferably, the mass volume ratio of the solid by-product obtained in described dry algae-residue or algae bio diesel oil refining process and water is 30%～80%.
Preferably, the solid obtained in described step (2) uses dehydrated alcohol and deionized water wash successively.
Principles of the invention: algae substances is catalytic pyrolysis under hydrothermal conditions, when cryogenic high pressure (in hermetic container steam high pressure) or suitably catalysis, algal biomass is through chemical reaction generation carbonizations such as dehydration, decarboxylation and condensations.
The invention have the advantages that
(1) preparation process of the present invention is simple, environmental friendliness, and product property is stable, and the activated carbon prepared can apply to the fields such as chemical fertilizer and pesticide action-controlling, soil improvement, air cleaning; Algae toxins efficient-decomposition can be removed by preparation process, alleviate the harm of Algae toxins; Material therefor algae-residue/algae mud or dry algae-residue and algae refine the side-product substantial amounts obtained, and wide material sources, are prone to collect.
(2) present invention directly utilizes the algae-residue/algae mud of high-moisture or dry algae-residue is that charcoal/activated carbon efficiently prepared by raw material, particularity due to raw material surface texture, prepare that surface is oxygen-containing, nitrogen-containing functional group, the biological activated carbon of structure-rich, part retains frustule surface features; Avoiding algae-residue early stage dehydration to consume energy, algae-residue is the release of toxic and harmful and GHG carbon dioxide in Pintsch process or natural decomposition process, thoroughly decomposes the cyanophycean toxin being difficult to dispose.
(3) the method utilizes algal biomass to prepare charcoal/activated carbon for material hydro-thermal carbonization, algal biomass cracking dehydration produces activated carbon under hydrothermal conditions, preparation process is substantially without additive, process equipment is simple, easy to operate, application scalable joint property is strong, it is to avoid chemical method prepares activated carbon complex operation, heavy-polluted shortcoming.
(4) the method can turn waste into wealth, and can dispose and be difficult to process water content height, bulky algae-residue/algae mud and contained toxin thereof, can prepare again eco-friendly Carbon Materials. The Carbon Materials simultaneously prepared can also be used in the fields such as wastewater treatment, air cleaning, soil remediation, fertilizer and pesticide controlled release, reaches the target of the treatment of wastes with processes of wastes against one another.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the biological activated carbon using the method for the embodiment of the present invention 1 to prepare.
Fig. 2 is the scanning electron microscope (SEM) photograph of the biological activated carbon using the method for the embodiment of the present invention 2 to prepare.
Fig. 3 is the ratio that mixes with water of algae-residue in the embodiment of the present invention 2/algae mud graph of a relation to biological activated carbon productivity.
Fig. 4 is ratio that in the embodiment of the present invention 3, dry algae powder mixes with the water graph of a relation to biological activated carbon productivity.
Detailed description of the invention
The reactor that hydro-thermal reaction of the present invention adopts refers to the miniature high pressure reaction still of hydrothermal reaction kettle that existing commercial production uses or use for laboratory.
Embodiment 1
Utilize the clay standby biological activated carbon of laboratory cultures blue algae
Comprise the following steps:
(1) centrifugal collection algae mud; Algae culture solution 400ml (algae density: 1～5 × 107Individual frustule every milliliter), 10000 leave the heart 10 minutes, abandon supernatant and collect precipitation, resuspended with 40ml deionized water.
(2) algae mud (water content about 90%) is inserted in 50ml hydrothermal reaction kettle (pressure is less than 6MPa) 160 DEG C～220 DEG C constant temperature carbonizations 2～20 hours in Electric heat oven, naturally cools to room temperature.
(3) by mixed liquor centrifugation in hydrothermal reaction kettle (9000 turns, 10 minutes), collect precipitation and use deionized water, washes of absolute alcohol three times successively, then dry at 50～60 DEG C, obtain the biological activated carbon shown in Fig. 1.
Embodiment 2
Directly utilize the clay standby biological activated carbon of algae-residue/algae
Comprise the following steps:
(1) blue-green algae residue/algae mud in Blue-green Algae Fast Growth period is salvaged.
(2) directly by 10g algae-residue/algae mud (water content is 90.5%) with mass volume ratio respectively 1:0; 3:1; 2:1; 1:1; 1:2; 1:3 is placed in 50ml hydrothermal reaction kettle (pressure is less than 6MPa) in Electric heat oven 160 DEG C～220 DEG C isothermal reactions 2～20 hours, naturally cools to room temperature.
(3) by mixed liquor centrifugation in hydrothermal reaction kettle (9000 turns, 10 minutes), collect precipitation and use deionized water, washes of absolute alcohol three times successively, then dry at 50～60 DEG C, obtain biological activated carbon as shown in Figure 2.
As shown in Figure 3, along with to the increase of amount of water in algae-residue/algae mud, the conversion ratio of biological activated carbon is gradually lowered (dropping to 8.7% from 14.9%), and prompting algae-residue/algae mud is directly inserted reactor without adding water and reacted the higher yields that can reach biological activated carbon.
Embodiment 3
The blue-green alga bloom algae-residue utilizing natural drying prepares biological activated carbon
Comprise the following steps:
(1) algae-residue of natural drying, size-reduced one-tenth dry algae powder are manually salvaged during breakout of cyanobacteria blooms.
(2) 2g dry algae powder is mixed from 5%～15% with mass volume ratio with water; 6g dry algae powder is mixed from 20%～200% with mass volume ratio with water. Being placed in 50ml hydrothermal reaction kettle (pressure is less than 6MPa) in Electric heat oven 160 DEG C～220 DEG C degrees Celsius constant temperature charcoals reacts 2～20 hours, naturally cools to room temperature.
(3) by mixed liquor centrifugation in hydrothermal reaction kettle (9000 turns, 10 minutes), collect precipitation and use deionized water, washes of absolute alcohol three times successively, then drying biological activated carbon at 50～60 DEG C.
As shown in Figure 4, along with to the increase of amount of water in dry algae powder, the conversion ratio of biological activated carbon gradually rises, continuing to increase the water yield, the conversion ratio of biological activated carbon is gradually lowered again.
Dry algae powder and the mixed proportion of water that biological activated carbon productivity is optimum are 30%～80%.
The foregoing is only the preferred embodiment of the invention; not in order to limit the invention; the any amendment made within all spirit in the invention and principle, equivalent replacement and improvement etc., should be included within the protection domain of the invention.
Claims (9)
1. the method that biological activated carbon is prepared in the hydro-thermal carbonization utilizing algae-residue/algae mud, it is characterised in that comprise the following steps:
(1) algae-residue/algae mud is mixed with water insert in reactor, at pressure less than 6MPa, 160 DEG C～220 DEG C reacting by heating 2～20 hours, naturally cool to room temperature; (2) being filtered or centrifugation by the hydrothermal product in step (1), the solid obtained washs;
(3) product after the washing in step (2) is dried process at 50 DEG C～60 DEG C, obtains biological activated carbon.
2. the method that biological activated carbon is prepared in hydro-thermal carbonization according to claim 1, it is characterized in that, described algae-residue/algae mud be by manually salvaging, machinery is salvaged, directly filtered, flocculation, coagulating sedimentation or pneumatically supported method obtain algae and water break out high concentration algae aqueous mixtures or the algae mud of generation.
3. the mass volume ratio of the method that biological activated carbon is prepared in hydro-thermal carbonization according to claim 2, it is characterised in that the water content of algae-residue/algae mud is 80%～95%, algae-residue/algae mud and water is 1:(0～3).
4. the method that biological activated carbon is prepared in hydro-thermal carbonization according to claim 3, it is characterised in that the mass volume ratio of algae-residue/algae mud and water is 3:1 or 2:1 or 1:1 or 1:2.
5. the method that biological activated carbon is prepared in hydro-thermal carbonization according to claim 1, it is characterised in that described algae-residue/algae mud is the product by obtaining after filtering and concentrating.
6. the method that biological activated carbon is prepared in hydro-thermal carbonization according to claim 5, it is characterised in that by Algae culture solution 400ml centrifugal 10min when 10000 turns, abandon supernatant and collect precipitation, resuspended with 40ml deionized water, obtain product.
7. the method that biological activated carbon is prepared in hydro-thermal carbonization according to claim 1, it is characterised in that described algae-residue/algae mud is the solid by-product obtained in the algae-residue dried or algae bio diesel oil refining process; The solid by-product obtained in described dry algae-residue or algae bio diesel oil refining process and the mass volume ratio of water are 5%～200%.
8. the method that biological activated carbon is prepared in hydro-thermal carbonization according to claim 7, it is characterised in that the solid by-product obtained in described dry algae-residue or algae bio diesel oil refining process and the mass volume ratio of water are 30%～80%.
9. the method that biological activated carbon is prepared in hydro-thermal carbonization according to claim 1, it is characterised in that the solid obtained in described step (2) uses dehydrated alcohol and deionized water wash successively.
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Cited By (13)
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| CN106475052A (en) * | 2016-11-16 | 2017-03-08 | 中国科学院烟台海岸带研究所 | A kind of application seaweed biomass prepares nano-sized magnesium hydroxide/N doping porous carbon composite material and preparation method thereof |
| CN107876020A (en) * | 2017-10-20 | 2018-04-06 | 福建省农业科学院农业生态研究所 | A kind of adsorbent, preparation method and applications |
| CN108059147A (en) * | 2017-12-27 | 2018-05-22 | 重庆文理学院 | A kind of method for preparing carbon material using discarded sunflower |
| WO2018113910A1 (en) * | 2016-12-20 | 2018-06-28 | Zenthoefer Rainer | Substrate and method for producing the substrate |
| CN108380178A (en) * | 2018-03-12 | 2018-08-10 | 秋晓东 | A kind of preparation method of restoration of the ecosystem agent and its absorbing process to radionuclide |
| CN108928906A (en) * | 2018-07-13 | 2018-12-04 | 南京师范大学 | Aluminate coagulating algae-residue prepares persulfate activator and method |
| CN109231634A (en) * | 2018-11-06 | 2019-01-18 | 江苏澳洋生态园林股份有限公司 | A kind of water body restoration device with algae water separation function |
| CN109231633A (en) * | 2018-11-06 | 2019-01-18 | 江苏澳洋生态园林股份有限公司 | A kind of red tide lash-up recovering method |
| CN109317100A (en) * | 2018-11-19 | 2019-02-12 | 长沙理工大学 | Normal-temperature pretreatment-hydrothermal carbonization method for preparing magnetic algae-based biochar |
| CN112028680A (en) * | 2020-08-21 | 2020-12-04 | 上海耀嵘环保科技有限公司 | Process for deeply treating eutrophic algae such as blue algae and extracting liquid fertilizer raw material |
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| CN114933926A (en) * | 2022-06-20 | 2022-08-23 | 无锡市检验检测认证研究院 | Device and method for converting blue algae into biomass black particles |
| CN115745688A (en) * | 2022-06-22 | 2023-03-07 | 杨粉莉 | Novel bio-organic fertilizer and preparation method thereof |
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Cited By (17)
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| CN106475052A (en) * | 2016-11-16 | 2017-03-08 | 中国科学院烟台海岸带研究所 | A kind of application seaweed biomass prepares nano-sized magnesium hydroxide/N doping porous carbon composite material and preparation method thereof |
| CN106475052B (en) * | 2016-11-16 | 2019-11-12 | 中国科学院烟台海岸带研究所 | A kind of application seaweed biomass prepares nano-sized magnesium hydroxide/N doping porous carbon composite material and preparation method thereof |
| WO2018113910A1 (en) * | 2016-12-20 | 2018-06-28 | Zenthoefer Rainer | Substrate and method for producing the substrate |
| CN107876020A (en) * | 2017-10-20 | 2018-04-06 | 福建省农业科学院农业生态研究所 | A kind of adsorbent, preparation method and applications |
| CN107876020B (en) * | 2017-10-20 | 2020-10-27 | 福建省农业科学院农业生态研究所 | Adsorbent, preparation method and application thereof |
| CN108059147A (en) * | 2017-12-27 | 2018-05-22 | 重庆文理学院 | A kind of method for preparing carbon material using discarded sunflower |
| CN108380178A (en) * | 2018-03-12 | 2018-08-10 | 秋晓东 | A kind of preparation method of restoration of the ecosystem agent and its absorbing process to radionuclide |
| CN108928906A (en) * | 2018-07-13 | 2018-12-04 | 南京师范大学 | Aluminate coagulating algae-residue prepares persulfate activator and method |
| CN109231633B (en) * | 2018-11-06 | 2021-07-16 | 江苏澳洋生态园林股份有限公司 | Red tide emergency restoration method |
| CN109231634A (en) * | 2018-11-06 | 2019-01-18 | 江苏澳洋生态园林股份有限公司 | A kind of water body restoration device with algae water separation function |
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| CN109231634B (en) * | 2018-11-06 | 2021-09-21 | 江苏澳洋生态园林股份有限公司 | Water body restoration device with algae-laden water separating function |
| CN109317100A (en) * | 2018-11-19 | 2019-02-12 | 长沙理工大学 | Normal-temperature pretreatment-hydrothermal carbonization method for preparing magnetic algae-based biochar |
| CN112094138A (en) * | 2020-08-21 | 2020-12-18 | 上海耀嵘环保科技有限公司 | Process for deeply treating eutrophic algae such as blue algae and extracting organic carbon source |
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